Apparatus for making chlorin.



Patented Dec. 4, I900. P. NAEF. APPARATUS FOR MAKING CHLORIN.

(Application med Apr. 24, 1900.1

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P. .NAEF.

APPARATUS FOR MAKING CHLORIN.

(Application filed Apr. 24, 1900.) (No Model.) 2 $heats8heet 2.

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Urrnio STATES PATENT PAUL NAEF, OF NEW YORK, N. Y.

APPARATUS FOR MAKING CHLORIN.

SPECIFICATION formingart of Letters Patent No. 663,088, dated Decenihei-4, 1960. Original application filed August 7, 1897, $erial No. 647,463.Divided and this application filed April 24, 1900. Serial (No model.)

To all whom it may concern.-

Be it known that I, PAUL NAEF, of N0. 132 Woody Crest avenue, near OneHundred and Sixty-fifth street, New York, in thecounty of New York andState of New York, have invented certain new and useful Improvements inApparatus for the Manufacture of Chlorin; and I do hereby declare thefollowing to be a full, clear, and exact description of the invention,such as will enable others skilled in the art to which it appertains tomake and use the same.

My invention relates to an improved apparatus for the manufacture ofchlorin, the same being shown and described in my application formanufacture of chlorin, Serial No. (547,463, filed August 7, 1897, ofwhich this application is a division, one object of the presentinvention being to provide means to effect the automatic and continuousproduction of chlorin from ammonium chlorid and magnesium oxid and toreduce the cost of the manufacture of chlorin to a minimum.

A further object is to provide an apparatus for the manufacture ofchlorin which shall be comparatively simple in construction, which shallbe automatic, continuous, and economical in operatipn, and which shallbe effectual in all respects in the performance of its functions.

With these objects in view the invention consists in certain novelfeatures of construction and combinations and arrangements of parts, ashereinafter set forth, and pointed out in the claims.

In the accompanying drawings, Figure 1 is a View of my improvedapparatus in position for use. Figs. 2 and 3 are sectional views of thefurnace, and Fig. l is a sectional view of the absorber.

My improved apparatus may be used in combination with the ammonia-sodaprocess. In the latter process brine saturated with ammonia is treatedwith carbonic-acid gas. Sodium bicarbonate is precipitated andammoniumchlorid and undecomposed salt are left in solution. From this solutionpure solid ammonium chlorid is produced by freezing or evaporation,which forms the raw material for the process to be hereinafterdescribed. A metallic oxid, preferably mag nesium oxid, is mixed bymechanical means with ammonium chlorid. This mixture is passedcontinuously through a retort-furnace. At the same time carbonic ornitrogen gas is drawn from the discharge end to the feed end thereof.This gas, containing ammonia-vapors, is drawn from the furnace throughcondensers, and a slight vacuum will be maintained in the wholeapparatus. The magnesium oxid, which has been partly con verted intomagnesium chlorid during the passage through the furnace, iscontinuously chargedinto another retort-furnace, prefer ably on a lowerlevel than the first and preferably of larger size. Heated air is passedinto the lower end of the lower furnace, and the oxygen of theatmosphere decomposes the magnesium chlorid, which is heated to darkredheat in the furnace. Ohlorin escapes from the higher end of the lowerfurnace, and magnesium oxid is discharged at the lower end of thefurnace and is again utilized in carrying outthe process. The reactionswhich take place in the upper furnace can be eX- pressed thus:

Ammonium chlorid is raised and deposited into a hopper 1 by means of anelevator 2, and magnesium oxid is elevated from a hopper 3 and depositedinto a hopper i, said hoppers l and 4 being preferably disposed side byside above the inlet or charging end of the upper furnace A. Screwconveyers 5 and 6 deliver the two materialsviz., ammonium chlorid andmagnesium oxid-into a hopper 7. The speed of the conveyers is soregulated that hopper 7 contains a mixture of chlorid and oXid suitablefor the process. A large excess of magnesium oXid over that required inthe above equation is used chiefly for the purpose of preventing asintering of the magnesium chlorid in the lower furnace and also for thepurpose of reaching a complete elimination of ammonia in the upperfurnace. The mixture of magnesium oxid and ammonium chlorid in hopper 7is so regulated that the material which is discharged from furnace Acontains one part of magnesium oXid to one to two parts of magnesiumchlorid. The am monia-gas escapes from the furnace A through a pipe 8into a cooler 9, comprising a cylinder containing a number of tubes. Thegas passes through the pipes or tubes 10 of the cooler, which aresurrounded by cold Water entering through a pipe 11 and having its exitat 12. The object of the cooler is to cool the gases and to remove anyammonium chlorid which may escape undecomposed. For this latter purposewarer is run into the top of the cooler through pipes 13 and allowed torun through the pipes or tubes 10 and wash out the ammonia and run offat 14:. To insure a complete condensation of the chlorid-vapors, thespaces 15 which water or any other absorbing liquid iscirculated. Inorder to assist the evolution and complete elimination of ammonia, a gasmay be circulated through the furnace and the condensing apparatus whichhas no decomposing action on ammonia and magnesium chlorid. Such a gasmay be obtained in the shape of waste gas in the ammoniasoda process andconsists mostly of nitrogen and contains some carbonic oxid and carbonicacid. Instead of the waste gas above mentioned gas from a limekiln orany other gas containing carbonic acidcan be used, inwhich case theammonia is obtained as carbonate. The apparatus is usually worked insuch a manner that always the same gas is circulating and only lossesare made up by drawing gas from a gas-holder connected with scrubber 17at 18. A pump 19 draws the gas from the scrubber 17 and delivers it tothe upper furnace A through a pipe 20. A slight vacuum will bemaintained in the whole apparatus. If the vacuum rises above one inch,(measured at the charging end of the furnace) gas will be drawn in at 18from the gas-holder, preferably through a reducing-valve of any preferred form of construction. The presence of oxygen in the gascirculating through the apparatus must be strictly avoided, because itwill destroy some of the ammonia. The gas discharge end of the furnace,because it is desirable to prevent moisture being retained in thematerial. The reason forintroducing steam between the ends of thefurnace or container in which the ammonia is involved is to hydrate themagnesium inthe cooler partsof the furnace, and thus facilitate thereaction, which can in this case be expressed:

It may be here stat-ed that ammonia can to a certain extent beeliminated without circulating gas or introducing steam; but the use ofthe latter is preferable both for preventing loss of ammonia and forfacilitating reaction.

The hoppers 1, 4, andiare connected at 22 to the pipe 8, leading intothe condensers, so as to draw off any am nionia-gas which may be evolvedfrom these vessels. All the elevators and hoppers are preferably made ofiron and are made air-tight.

The gas circulating through the apparatus can be heated in Cowper orother stoves before entering the furnace at A6, and thus all or part ofthe heat necessary for the reaction can besupplied in this way. v If asufficient volume of gas free from oxygen can be easily procured tosupply all the heat, a furnace with a solid lining instead of with alining constructed with heating-fines might be used.

The furnace A is the same in construction as the furnace B, which isused for the evolution of chlorin and a detailed discription of whichwill be hereinafter given; but the furnace A is smaller than furnace B.

' Instead of arranging the furnace A above the furnace 13 both furnacesmay bedisposed on the same plane, if desired; but this would require anadditional hopperand elevator to raise the material into hopper 2 L.

As stated when describing the action of furnace A, part or all the heatcan be supplied also to furnace B' by preheating the air in hotairstoves. In such cases, and especially if an excess of air is notobjectionable, such as in the manufacture of chlorate of potash, wherethe chlorin is absorbed by milk of lime, furnaces with solid lining canbe used.

The material which is continuously discharged from furnace A consists ofmagnesium chlorid and oxid and runs continuously into hopper 24, fromwhich it is continuously fed into'furnace B by means of a conveyer 25.In the furnace B chlorin is evolved by the action of oxygen on thechlorid. The reactions in thelower furnace may be expressed as follows:

The magnesium oxid which is formed in the furnace B is contin uouslydischarged from the furnace into hopper 3,from Wl'llGhll; is elevated tohopper 1, as previously explained. Air enters thefurnace B at 26, andchlorin-gasleaves it at 27. The chlorin-gas passes through two scrubbers28 28 into a chlorin-absorber C, where it is absorbed by lime andisconvertedinto-bleaching-powder. Withtheabsorber a suction fan orpump'29 is connected and serves to draw off the waste gases and createsa slight vacuum in the entire apparatus, as above intimated.

The scrubbers 28 28 are of the ordinary construction used inehlorin-works. In the first scrubber any hydrochloric acid is washed outby water, and in the second scrubber the chlorin-gas is dried by meansof strong sulfuric acid. At thesame time the is cooled (by radiation)during passage through pipes and scrubber. 1

Each furnace A and B is revolubly mounted and provided with flues 30 inthe periphery, which fines may be conveniently formed by channeled tiles31. Each furnace is provided with lifting partitions 32 for agitating orshowering the material. Each furnace is also provided with afire-chamber 33 at one end, said fire-chamber having perforated crowns34 35, beneath which a gas-jet 36 is projected. Two flue-rings 37 38 arelocated on the periphery of the furnace, the one near the discharge endhaving com munication with the fire-chamber and the one near the inletor charge end of the furnace being in communication with the chimney 39.The annular flueset) extend around the periphery and are preferablyformed by two rings spaced apart and encircled bya ring 41, which restson the pedestal, said" ring 41 being also made in two parts securedtogether; By this arrangeinent ready access may be had to the annularfines, the latter being always in communication with the longitudinalflues 30. The firegases pass from the fire-chamber through the.perforated crowns into the annu lar flues and thence through thelongitudinal flues. The furnace carries at the charging end a plate 42,against which astationary plate 43 is located, and through the latterthe conveyers and the gas-pipe enter, said gas pipe or furnace B beinglettered 4:4: in the drawings. The plate 43 is made of as small diameteras possible, so as to reduce leakage to a minimum. The discharge end ofthe furnace is closed by a plate 45, to which is fastened theentrance-pipe 20 of furnace A and 26 of furnace B. The pipe 20 (furnaceA) is connected by a turning joint 47 with the stationary main. Thematerial is discharged from the respective furnaces through holes 48 inthe plate 45. To prevent leakage of gas, a stationary hollow orchambered ring 49 is made to bear closely against the plate 45 andcommunicate with all the holes therein. The hollow rings 49 areconnected by suitable pipes with the hoppers below them.

Each revoluble furnace A B is supported by rollers 50 and kept inposition by means of V-shaped rollers 51. Thefurnaces may be slowlyrevolved by means of worm-gear orin any preferred mannei.

The chlorin-absorber O hereinbefore referred to consists, preferably, ofan iron cylinder mounted andrevolvediu the same manner as the furnaces Aand B. The absorber is fitted with iron pipes 52, which run through theend plates 53 54, and these pipes act in two ways. They lift and showerthe lime and they are also used for cooling to carry off the heat formedby the combination of lime and chlorin. For this purpose the pipes areopen at both ends, so as to allow a free How of air through them. Thedischarge end of the absorber is surrounded by a casing 55, which is inconnection with a chimney toincrease the draft. If necessary, water canbe circulated through these pipes. The cylinder is also fitted withradial lifting partitions 56. The charging end of the absorber is thesame as the furnaces A and B. Lime is continuously fed from. a hopper 57through conveyer 58 into the absorber and leaves it as bleachingpowderat 59.

My improved apparatus can be'used for decomposing chlorid of magnesiumobtained from other sources than by decomposing chlorid of am monia. Inthis case the furnace A is unnecessary and the arrangementof furnace Bis exactly as described, the only difference being that the hoppers land 4 and miXing-conveyeis 5 and 6 are placed above the hopper 24. Thehopper 1 contains in that case magnesium chlorid instead of ammouiu n1chlorid. The con veyers 5 and 6 will be so regulated that the hopper 24contains a material of similar composition as when decomposing ammoniumchlorid. The magne sium oXid produced in furnace B can then be used inother industries.

The hoppers 2-11: and 3 are used so that furnace B can be operated during short stoppages of furnace A, and vice versa.

Having fully described my invention, what Iclaim as new, and desire tosecure by Letters Patent, is

1. The combination with a furnace, of a hopper communicating therewith,two hoppers communicating with said first-mentioned hopper, a gas-outletat one end of said furnace, a discharge-pipe communicating with theother end of said furnace, and means for injecting a gas into the outletend of said furnace, substantially as set forth.

2. The combination with a furnace, of two hoppers for containing chloridof ammonium and oXid of magnesium respectively, a third hopper adaptedto receive said chemicals from the first-mentioned hoppers and dischargethem into the furnace, a pipe for conducting ammonia from the furnaceand pipes connected with said ammonia-pipe and communicating with thehoppers so as to receive ammonia from the latter, substantially as setforth.

3. The combination with a furnace and means for mixing chlorid ofammonium and oxid of magnesium and discharging the same into saidfurnace, of a pipe for conducting ammonia from the furnace, and a washerwith which said pipe communicates, said washer comprising a cylinder,aseries of pipes therein, absorbent material in the cylinder above andbelow said pipes and means for discharging water into the top of thecylinder, substantially as set forth.

4. The combination with a revoluble cylinder having a number ofindependent l0ngitudinal peripheral fines or passages, an annular fineor passage encircling said cylinder and communicating with thelongitudinal flues or passages, a furnace communicating with saidannular flue or passage, another annular flue or passage encircling theother end of the cylinder and communicating with said independentlongitudinal fines and a stack communicating with said last-mentionedannular flue or passage, substantially as set forth.

5. The combination with a revoluble cylinder having a number ofindependent longitudinal peripheral fiues, a series of rings securedtogether and encircling one end of said cylinder and forming an annularflue com-' municating with the longitudinal fiues, a furnacecommunicating with said annular flue, another series of rings securedtogether and encircling the other end of the cylinder and forminganother annular flue communicating with said independent longitudinallines and a stack communicating with said last-mentioned annular flue,substantially as set forth.

6. The combination with a revoluble furnace, of a ring secured to andpartially closing one end thereof, so as to leave a small opening, asmall fixed plate abutting against said ring supported independently ofthe furnace and cooperating with said ring to close the small opening inthe end of the furnace and inlet and outlet devices communicating Withthe furnace through said small fixed plate, substantially as set forth.

7. The combination with a revoluble furnace, of two hoppers forcontaining chlorid of ammonium and oxid of magnesium respectively, athird hopper communicating with the first two and with the furnace, apipe for discharging gas into the discharge end of the furnace, a pipefor conducting ammonia from the inlet end of the furnace, a secondfurnace, a hopper communicating therewith,

means for conducting the mixture of chlorid and oxid of magnesium fromthe first furnace to said last-mentioned hopper, means for injecting airinto said second furnace, a hopper communicating with said secondfurnace to receive oxid of magnesium therefrom, an elevator forconveying oxid of magnesium from said last-mentioned hopper to one ofthe firstmentioned hoppers, a chlorin-absorber and a pipe for conductingchlorin from said second furnace to said'absorber, substantially as setforth.

8. The combination with a revoluble furnace and a pipe communicatingWith the discharge end thereof, of two hoppers for 'containing chloridof ammonium and oxid of magnesium respectively, a third hopper, twoconveyers for conducting the chemicals from the first-mentioned hoppersinto the third hopper, and a conveyer for conducting the mixed chemicalsfrom the third hopper to the furnace.

9. The combination with a cylinder mounted to revolve, of a stationaryhollow ring closing against the end plate of the cylinder, said endplate having holes communicating with the interior of the cylinder andwith the chamber in the stationary hollow ring and means for conductingmaterial from the chamber of said hollow ring.

10. In an apparatus for making chlorin, the combination with a furnace,of a washer communicating therewith, said Washer comprising a cylinderhaving layers of material therein for bringing gas and liquid intointimate contact, means for conducting gas from the furnace to saidcylinder, means for discharging Water into said cylinder, andcooling-pipes in the cylinder.

In testimony whereof I have signed this specification in the presence oftwo subscribing witnesses.

PAUL NAEF.

Witnesses:

O. E. LANGDON, GERRIT SMITH.

